Dichlorodiphenylsilane → HCID 4351769、化合物

HRID 1906292

反応式

HRID 1906292 の反応式
[CH2:1]([Mg]Br)[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][CH2:16][CH2:17][CH3:18].Cl[Si:22](Cl)([C:29]1[CH:34]=[CH:33][CH:32]=[CH:31][CH:30]=1)[C:23]1[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=1>>[CH2:1]([Si:22]([CH2:18][CH2:17][CH2:16][CH2:15][CH2:14][CH2:13][CH2:12][CH2:11][CH2:10][CH2:9][CH2:8][CH2:7][CH2:6][CH2:5][CH2:4][CH2:3][CH2:2][CH3:1])([C:29]1[CH:34]=[CH:33][CH:32]=[CH:31][CH:30]=1)[C:23]1[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=1)[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][CH2:16][CH2:17][CH3:18]

参加物

3

反応物 2

HCID 6627Dichlorodiphenylsilane2 回HCID 178442890HCID 178442890、化合物

生成物 1

HCID 4351769HCID 4351769、化合物収率 78%

実験手順

The first portion of the octadecylmagnesium bromide was cooled to 0° and cuprous cyanide (0.12 g 1.34 mmoles) was added with stirring. Then dichlorodiphenylsilane (1.95 ml, 9.27 mmoles) was added. The reaction mixture was stirred at 10° for 140 minutes. Gas chromatographic analysis showed that most of the dichlorodiphenylsilane had disappeared during the first hour of reaction. The mixture was then stirred at room temperature for about 16 hours (i.e. overnight). The reaction mixture was then filtered, quenched with water, and acidified slightly with HCl. After extraction with diethylether, drying (with MgSO4) and removal of solvent, a solid was obtained. Extraction with hot heptane and crystallization provided 4.96 g of dioctadecyldiphenylsilane. The yield was about 78%.

後処理

  1. stirringThe reaction mixture was stirred at 10° for 140 minutes
  2. customhad disappeared during the first hour of reaction
  3. stirringThe mixture was then stirred at room temperature for about 16 hours (i.e. overnight)
  4. filtrationThe reaction mixture was then filtered
  5. customquenched with water
  6. extractionAfter extraction with diethylether
  7. customdrying
  8. custom(with MgSO4) and removal of solvent
  9. customa solid was obtained
  10. extractionExtraction
  11. customwith hot heptane and crystallization

出典と根拠

ORDレコード
ord-965c22f5de6a4bfa9e31a0a5b952a12b
出典データセット
uspto-grants-1987_03
特許番号
US04650891

関連ノート

読み込み中…